Sukhanova A M, Perova I B, Koshechkina A S, Rylina E V, Tumolskaya E V, Rodionova G M
Federal Research Centre of Nutrition, Biotechnology and Food Safety, 109240, Moscow, Russian Federation.
I.M. Sechenov First Moscow State Medical University (Sechenov University), 119991, Moscow, Russian Federation.
Vopr Pitan. 2020;89(6):123-129. doi: 10.24411/0042-8833-2020-10085. Epub 2020 Nov 20.
Sibutramine is a highly effective drug for the treatment of obesity. In this regard, unscrupulous manufacturers can add sibutramine as a biologically active synthetic substance prohibited for use in the composition of dietary supplements. Thus, the problem associated with the illegal circulation of such dietary supplements is especially actual, given the scale of the sale of these products. The development and validation of methods for the determination of sibutramine in dietary supplements for slimming (anorexigenic action) for the purpose of quality control in order to ensure the quality of dietary supplements when introduced into civil circulation at customs and on the market. of the study - to develop a method for the quantitative determination of sibutramin in dietary supplements for weight loss by high performance liquid chromatography (HPLC) and to validate it. . For the quantitative determination of sibutramine in dietary supplements, we used an Agilent 1100 high performance liquid chromatograph with a UV-detector. The stationary phase was a chromatographic column C NUCLEOSIL 4.6×150 mm, particle size 5 μm. The mobile phase contained 0.05 M formate buffer pH 4.0 and acetonitrile in a ratio of 40:60 (by volume). . A methodology has been developed for the determination of sibutramine in dietary supplements for weight loss, which makes it possible to control the quality of dietary supplements. Based on the obtained chromatograms, the specificity was determined; the plant components did not influence the determination of sibutramine in model mixtures. The suitability of the chromatographic system was determined: the retention factor of the compound - 2.222 (more than 2.0), N - 5776 theoretical plates (more than 5000), T peak of sibutramine - 0.939 (not more than 1.5). Within the analytical area of the linearity method: R=0.9993 (over 0.9950). ε=0.46% (does not exceed 1.5%), the confidence interval includes the value of 100%, the calculated value of the Student's criterion tcalc (2.47) was less than the tabular ttable (2.80), which proved the correctness of the methodology. The precision of the results was determined by the obtained RSD value, which was 0.91% (less than 1%). Limit of detection (LOD) and limit of quantification (LOQ) took values of 0.1 and 1.0%, respectively. The range of measured concentrations was 0.01-20.0 mg/g. . As a result of the studies, the method for sibutramine determination in dietary supplements with anorexigenic action was tested and can be used in quality control of dietary supplements.
西布曲明是一种治疗肥胖症的高效药物。在这方面，无良制造商可能会在膳食补充剂成分中添加西布曲明这种被禁止使用的生物活性合成物质。因此，鉴于此类产品的销售规模，与这类膳食补充剂非法流通相关的问题尤为突出。为了在海关和市场上确保膳食补充剂投入民用流通时的质量，开展并验证用于测定具有减肥（食欲抑制作用）功效的膳食补充剂中西布曲明的方法以进行质量控制。本研究的目的是开发一种通过高效液相色谱法（HPLC）定量测定减肥膳食补充剂中西布曲明的方法并进行验证。为了定量测定膳食补充剂中的西布曲明，我们使用了配备紫外检测器的安捷伦1100高效液相色谱仪。固定相为色谱柱C NUCLEOSIL 4.6×150 mm，粒径5μm。流动相包含0.05 M pH 4.0的甲酸盐缓冲液和乙腈，比例为40:60（体积比）。已开发出一种用于测定减肥膳食补充剂中西布曲明的方法，该方法能够控制膳食补充剂的质量。根据所得色谱图确定了特异性；植物成分不影响模型混合物中西布曲明的测定。确定了色谱系统适用性：化合物的保留因子为2.222（大于2.0），理论塔板数N为5776（大于5000），西布曲明的峰拖尾因子T为0.939（不超过1.5）。在线性方法的分析范围内：R = 0.9993（大于0.9950）。ε = 0.46%（不超过1.5%），置信区间包含100%的值，计算得到的学生准则tcalc值（2.47）小于表格中的ttable值（2.80），这证明了该方法的正确性。通过所得相对标准偏差（RSD）值确定结果的精密度，其为0.91%（小于1%）。检测限（LOD）和定量限（LOQ）分别为0.1%和1.0%。测量浓度范围为0.01 - 20.0 mg/g。研究结果表明，用于测定具有食欲抑制作用的膳食补充剂中西布曲明的方法经过了测试，可用于膳食补充剂的质量控制。
